EP0041002A2 - Process for treating vegetable oils to improve their stability in the cold state - Google Patents
Process for treating vegetable oils to improve their stability in the cold state Download PDFInfo
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- EP0041002A2 EP0041002A2 EP81400750A EP81400750A EP0041002A2 EP 0041002 A2 EP0041002 A2 EP 0041002A2 EP 81400750 A EP81400750 A EP 81400750A EP 81400750 A EP81400750 A EP 81400750A EP 0041002 A2 EP0041002 A2 EP 0041002A2
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- 238000000034 method Methods 0.000 title claims abstract description 34
- 235000015112 vegetable and seed oil Nutrition 0.000 title claims abstract description 5
- 239000008158 vegetable oil Substances 0.000 title claims abstract description 5
- 239000003921 oil Substances 0.000 claims abstract description 79
- 235000019198 oils Nutrition 0.000 claims abstract description 77
- 239000013078 crystal Substances 0.000 claims abstract description 20
- 150000001875 compounds Chemical class 0.000 claims abstract description 10
- 239000006260 foam Substances 0.000 claims abstract description 9
- 238000010908 decantation Methods 0.000 claims abstract description 7
- 238000002425 crystallisation Methods 0.000 claims abstract description 4
- 230000008025 crystallization Effects 0.000 claims abstract description 4
- 239000001993 wax Substances 0.000 claims description 20
- 230000007935 neutral effect Effects 0.000 claims description 8
- 239000000344 soap Substances 0.000 claims description 6
- 239000002671 adjuvant Substances 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 3
- 238000012958 reprocessing Methods 0.000 claims description 2
- 239000007789 gas Substances 0.000 abstract description 10
- 239000011261 inert gas Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 238000001914 filtration Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 235000019486 Sunflower oil Nutrition 0.000 description 4
- 238000005352 clarification Methods 0.000 description 4
- 238000007670 refining Methods 0.000 description 4
- 239000002600 sunflower oil Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000035800 maturation Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 235000005687 corn oil Nutrition 0.000 description 2
- 239000002285 corn oil Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000008157 edible vegetable oil Substances 0.000 description 2
- 125000005456 glyceride group Chemical group 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000000080 wetting agent Substances 0.000 description 2
- 229920000715 Mucilage Polymers 0.000 description 1
- 235000019483 Peanut oil Nutrition 0.000 description 1
- 241000209504 Poaceae Species 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003925 fat Substances 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- -1 for example Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 239000000312 peanut oil Substances 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B7/00—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils
- C11B7/0075—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils by differences of melting or solidifying points
Definitions
- the subject of the present invention is a process for treating vegetable oils for improving their cold stability. This process makes it possible to clarify (for example by dewaxing, wintering) oils and in particular edible oils, such as for example, sunflower oil, corn oil, or peanut oil.
- the oil is cooled for a few hours to an appropriate temperature, making it possible to obtain crystals which can be separated by filtration.
- An adjuvant is often used filtration (for example filtering earth).
- the second method mentioned requires the use of a large quantity of wetting agent solution (5 to 10%) and the use of an expensive separation material and requiring high maintenance costs.
- the object of the present invention is to overcome these drawbacks by proposing a process making it possible to obtain clear oils even from oils having high levels of constituents with a high melting point (waxes, partial glycerides, etc.) without the use of filtration and centrifugation soils.
- This process is characterized in that, in a first step, the oil to be treated is cooled to a chosen temperature so as to allow the crystallization of the compounds to be eliminated, then in a second step, the oil thus treated is brought into a decanting container and subjected to the action of fine bubbles of a neutral gas which binds to these crystallized compounds so as to produce a foam with a density lower than that of oil.
- the gas-bubble crystal complex formed rises to the surface of the container, thus making it possible to obtain, at the bottom of the latter, after decantation, a clarified oil having a content of less than 30 ppm of crystals and with a yield greater than 90 %.
- the performance of such a process essentially depends on the formation of crystals of an appropriate size, a sufficient quantity of fine gas bubbles, in the liquid, and on the adhesion of the bubbles to the solid particles.
- a small amount of clarification aid is added to the oil to be treated, making it possible to reduce the affinity of the crystals with respect to the oily phase.
- the oil to be treated is a neutralized oil containing know, the latter fulfilling the function of clarifying adjuvants.
- the presence of water and active tension (soaps) promotes the adhesion of waxes to air bubbles.
- the gas-oil contact under pressure is carried out with stirring for a period of approximately 30 min.
- the method comprises a step of reprocessing the waxes making it possible to recover the oils which are contained therein.
- the oil to be treated is brought according to arrow A in a cooler 1 comprising an agitator 2.
- the oil to be treated is brought to the appropriate temperature, chosen according to the type of oil to be treated .
- the oil is then brought to a ripener 3 where it is kept at the same temperature so as to allow quantitative crystallization of the compounds to be removed, under conditions appropriate according to the type of oil.
- the oil is also subjected to agitation by means of an agitator 4.
- the oil is brought along arrow D to the lower part of a decantation container 5 and, it is subjected to the action of fine bubbles of a neutral gas, which attach to the crystals to eliminate so as to produce a gas-crystal complex in the form of a foam with a density lower than that of oil.
- This complex collects in zone 6 of the container, where it is removed by scraping according to arrow C.
- the production of fine bubbles of neutral gas is obtained by taking a fraction E of clarified oil which is brought into a saturator 8, where it is subjected to the action of a neutral gas such as air or nitrogen arriving according to arrow F under a pressure between 4 and 10 bars, before being expanded to atmospheric pressure, the duration of the gas-oil contact in the saturator 8 being approximately equal to 30 min.
- a neutral gas such as air or nitrogen arriving according to arrow F under a pressure between 4 and 10 bars
- a clarified oil G is recovered, a fraction E of which is recycled to the saturator 8.
- the flow rate of this fraction can range up to 300% of the flow rate of the oil to be treated leaving the ripener 3.
- This oil enriched in waxes can be treated by the method according to the invention or by usual methods (decantation, centrifugation, filtration).
- the starting raw material is a sunflower oil containing 800 ppm of waxes.
- This oil which has been subjected beforehand to neutralization and contains 0.4% of water and 1080-ppm of sodium hydroxide soap, it is introduced into a 5-liter beaker, equipped with an agitator. , all placed in a refrigerated enclosure at 5 ° C for a period of approximately 10 hours with continuous stirring.
- This oil is transferred to a saturator of 4 liters equipped with an agitator. The saturator is subjected to a pressure of 10 bars.
- the contacting time is 30 min with permanent stirring, the oil temperature being maintained at 5 ° C. by a coil located inside the reactor. At the end of this operation, the oil is expanded to atmospheric pressure by direct transfer to a 4-liter beaker. After one hour of decantation at + 5 ° C, a separation of two phases is obtained. At the bottom of the container, approximately 2,850 g of the dewaxed oil are recovered, which now contains only 20 ppm of waxes and 0.1% of water. At the top of the container, about 150 g of foam is recovered, consisting of a wax-fine gas bubble complex.
- the dewaxed oil can either be subjected to the following stages of refining, or subjected to a new treatment cycle in order to perfect the dewaxing process.
- the starting raw material is a sunflower oil containing 85 ppm of waxes. We take 3 kg of this oil previously neutralized and containing 0.3% water and 1400 ppm of sodium soap. By applying the method of Example 1, a dewaxed oil is obtained containing 7 ppm of waxes, 0.05% water and 52 ppm of soap. The yield of dewaxed oil is 98.4%.
- the starting oil is a new sunflower oil marked and discolored, containing 700 ppm of waxes, less than 0.05% water and less than 2 ppm of sodium.
- the procedure is the same as in Example 1.
- a dewaxed oil is obtained containing about 60 ppm of residual waxes with a yield greater than 93% of dewaxed oil.
- the starting oil is a crude corn oil containing 150 ppm of waxes.
- the procedure is as indicated in Example 1.
- a dewaxed oil is obtained containing 50 ppm of residual waxes and from which the suspended matters such as mucilages, solid particles, etc. are at the same time partially removed.
- the yield of dewaxed oil after clarification is therefore 95% and can range up to approximately 98.5%.
- oils obtained in Examples 1 to 5 are subjected to conventional refining operations as the case may be, up to the stage before deodorization.
- the samples thus obtained are stored at + 5 ° C for 24 hours or more.
- An oil containing 1% of waxes from dewaxing foams obtained by the process according to the invention is cooled to 25-30 ° C overnight and then centrifuged.
- the heavy phase containing the waxes represents 12% of the oil thus treated.
- the light fraction represents approximately 88% partially dewaxed oil at 400 ppm of waxes, which can be recycled as a mixture with the oil to be treated.
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Fats And Perfumes (AREA)
Abstract
Description
Procédé de traitement des huiles végétales pour l'amélioration de leur stabilité à froid.Process for treating vegetable oils to improve their cold stability.
La présente invention a pour objet un procédé de traitement des huiles végétales pour l'amélioration de leur stabilité à froid. Ce procédé permet de clarifier (par exemple par décirage, wintérisation) des huiles et notamment des huiles alimentaires, telles que par exemple, l'huile de tournesol, de mais, ou d'arachide.The subject of the present invention is a process for treating vegetable oils for improving their cold stability. This process makes it possible to clarify (for example by dewaxing, wintering) oils and in particular edible oils, such as for example, sunflower oil, corn oil, or peanut oil.
Il est bien connu que certaines huiles alimentaires deviennent troubles à cause de la présence de composés à haut point de fusion tels que cires, glycérides partiels, etc... qui cristallisent. Or, la présence de tels composés, si elle n'affecte en aucune façon la qualité de l'huile, altère nettement son aspect, et donc diminue son attrait pour le consommateur.It is well known that certain edible oils become cloudy due to the presence of compounds with a high melting point such as waxes, partial glycerides, etc. which crystallize. However, the presence of such compounds, if it does not in any way affect the quality of the oil, markedly alters its appearance, and therefore decreases its appeal to the consumer.
En conséquence, il est courant de faire subir à ces huiles, avant de les commercialiser, une opération de clarification, ayant pour but de parvenir à l'élimination des composés cristallisés.Consequently, it is common to subject these oils, before marketing them, to a clarification operation, the aim of which is to achieve the elimination of the crystallized compounds.
Pour effectuer cette opération de clarification, on utilise habituellement deux procédés de type classique.To carry out this clarification operation, two conventional methods are usually used.
Selon le premier de ces procédés, l'huile est refroidie pendant quelques heures à une température appropriée, permettant d'obtenir des cristaux pouvant être séparés par filtration. On utilise souvent un adjuvant de filtration (par exemple terres filtrantes).According to the first of these methods, the oil is cooled for a few hours to an appropriate temperature, making it possible to obtain crystals which can be separated by filtration. An adjuvant is often used filtration (for example filtering earth).
Selon le second de ces procédés, après précipitation des cristaux comme ci-dessus, on procède à une centrifugation d'un mélange de cette huile avec une solution aqueuse d'agent mouillant. De cette façon, on favorise le passage des cristaux dans la solution aqueuse, qui se sépare de l'huile par centrifugation.According to the second of these methods, after precipitation of the crystals as above, a mixture of this oil is centrifuged with an aqueous solution of wetting agent. In this way, the passage of the crystals in the aqueous solution, which separates from the oil by centrifugation, is favored.
Toutefois, ces procédés ne sont pas sans présenter de nombreux inconvénients.However, these methods are not without many drawbacks.
En effet, pour le premier procédé cité :
- - la difficulté d'obtenir des cristaux filtrables nécessite des cycles de refroidissement et de maturation de longue durée,
- - la capacité de production est fonction de la teneur en cristaux, elle peut diminuer d'environ 20 à 30 % lorsque la teneur en cristaux double, ce qui est courant dans la pratique industrielle,
- - ce procédé nécessite, en outre, l'emploi de terres filtrantes coûteuses qui en plus donnent des gâteaux de filtration pouvant contenir jusqu'à 60 % d'huile entraînée d'où des pertes importantes en huile raffinée. Ces gâteaux posent un problème de pollution de l'environnement (danger d'une inflammabilité spontanée à la suite de l'oxydation des graisses contenues et pollution de la nappe phréatique par la matière grasse par entraînement de celle-ci dans les eaux pluviales).
- - the difficulty of obtaining filterable crystals requires long-term cooling and maturation cycles,
- - the production capacity is a function of the crystal content, it can decrease by around 20 to 30% when the crystal content doubles, which is common in industrial practice,
- - This process requires, in addition, the use of expensive filtering earths which in addition give filter cakes which can contain up to 60% of entrained oil hence significant losses in refined oil. These cakes pose a problem of environmental pollution (danger of spontaneous flammability following the oxidation of the fats contained and pollution of the water table by fatty matter by entrainment of the latter in rainwater).
Par ailleurs, le deuxième procédé cité exige l'emploi d'une quantité de solution d'agent mouillant importante (5 à 10 %) et l'emploi d'un matériel de séparation coûteux et nécessitant des frais d'entretien élevés.Furthermore, the second method mentioned requires the use of a large quantity of wetting agent solution (5 to 10%) and the use of an expensive separation material and requiring high maintenance costs.
La présente invention a pour objet de pallier à ces inconvénients en proposant un procédé permettant d'obtenir des huiles claires même à partir d'huiles ayant des taux importants de constituants à point de fusion élevé (cires, glycérides partiels, etc..) sans utilisation de terres de filtration ni de centrifugation.The object of the present invention is to overcome these drawbacks by proposing a process making it possible to obtain clear oils even from oils having high levels of constituents with a high melting point (waxes, partial glycerides, etc.) without the use of filtration and centrifugation soils.
Ce procédé est caractérisé en ce que, dans une première étape, on refroidit l'huile à traiter à une température choisie de manière à permettre la cristallisation des composés à éliminer, puis dans une seconde étape, on amène l'huile ainsi traitée dans un récipient de décantation et on la soumet à l'action de fines bulles d'un gaz neutre qui se fixe à ces composés cristallisés de façon à produire une mousse de masse volumique inférieure à celle de l'huile. Le complexe cristaux-bulles de gaz formé monte à la surface du récipient, permettant ainsi d'obtenir à la partie inférieure de ce dernier, après décantation, une huile clarifiée ayant une teneur inférieure à 30 ppm de cristaux et avec un rendement supérieur à 90 %.This process is characterized in that, in a first step, the oil to be treated is cooled to a chosen temperature so as to allow the crystallization of the compounds to be eliminated, then in a second step, the oil thus treated is brought into a decanting container and subjected to the action of fine bubbles of a neutral gas which binds to these crystallized compounds so as to produce a foam with a density lower than that of oil. The gas-bubble crystal complex formed rises to the surface of the container, thus making it possible to obtain, at the bottom of the latter, after decantation, a clarified oil having a content of less than 30 ppm of crystals and with a yield greater than 90 %.
Les performances d'un tel procédé dépendent essentiellement de la formation de cristaux d'une taille appropriée, d'une quantité suffisante de fines bulles de gaz, dans le liquide, et de l'adhésion des bulles sur les particules solides.The performance of such a process essentially depends on the formation of crystals of an appropriate size, a sufficient quantity of fine gas bubbles, in the liquid, and on the adhesion of the bubbles to the solid particles.
Selon l'invention, on a obtenu des résultats particulièrement intéressants, en soumettant au moins une partie de l'huile refroidie préalablement jusqu'à précipitation quantitative des cristaux, à une pression de 4 à 10 bars de gaz neutre, et ensuite à une détente à la pression atmosphérique. Ces conditions particulières permettent d'obtenir des bulles de gaz dont la quantité et le diamètre sont tels qu'ils favorisent la formation quantitative d'un complexe bulles-cristaux de masse volumique inférieure à celle de l'huile.According to the invention, particularly advantageous results have been obtained, by subjecting at least part of the oil, cooled beforehand until quantitative precipitation of the crystals, to a pressure of 4 to 10 bars of neutral gas, and then to an expansion at atmospheric pressure. These particular conditions make it possible to obtain gas bubbles the quantity and diameter of which are such that they favor the quantitative formation of a bubble-crystal complex with a density lower than that of the oil.
Selon une variante du procédé, on ajoute à l'huile à traiter une faible quantité d'adjuvant de clarification permettant de diminuer l'affinité des cristaux vis-à-vis de la phase huileuse.According to a variant of the process, a small amount of clarification aid is added to the oil to be treated, making it possible to reduce the affinity of the crystals with respect to the oily phase.
Selon une autre caractéristique de l'invention, l'huile à traiter est une huile neutralisée contenant des savons, ces derniers remplissant la fonction d'adjuvants de clarification. En effet, on s'est aperçu que la présence d'eau et de tension-actifs (savons) favorise l'adhésion des cires aux bulles d'air.According to another characteristic of the invention, the oil to be treated is a neutralized oil containing know, the latter fulfilling the function of clarifying adjuvants. In fact, we have noticed that the presence of water and active tension (soaps) promotes the adhesion of waxes to air bubbles.
D'une façon préférentielle, le contactage gaz-huile sous pression s'effectue sous agitation pendant une durée d'environ 30 mn.Preferably, the gas-oil contact under pressure is carried out with stirring for a period of approximately 30 min.
Par ailleurs, et selon une autre caractéristique de l'invention, le procédé comporte une étape de retraitement des cires permettant de récupérer les huiles qui y sont contenues.Furthermore, and according to another characteristic of the invention, the method comprises a step of reprocessing the waxes making it possible to recover the oils which are contained therein.
Le procédé qui fait l'objet de l'invention peut fonctionner en continu ou en discontinu et sera décrit plus en détail en se référant à la figure annexée qui est un schéma de principe du fonctionnement en continu.The process which is the subject of the invention can operate continuously or batchwise and will be described in more detail with reference to the appended figure which is a block diagram of continuous operation.
Selon la figure, on amène l'huile à traiter selon la flèche A dans un refroidisseur 1 comportant un agitateur 2. Dans ce refroidisseur 1, l'huile à traiter est amenée à la température appropriée, choisie selon le type d'huile à traiter. A la sortie de ce refroidisseur, l'huile est ensuite amenée à un maturateur 3 où elle est maintenue à la même température de manière à permettre la cristallisation quantitative des composés à éliminer, dans des conditions appropriées selon le type d'huile. Pendant cette étape de maturation, l'huile est également soumise à une agitation au moyen d'un agitateur 4.According to the figure, the oil to be treated is brought according to arrow A in a
Au sortir du maturateur 3, on amène l'huile selon la flèche D à la partie inférieure d'un récipient de décantation 5 et, on la soumet à l'action de fines bulles d'un gaz neutre, qui se fixent aux cristaux à éliminer de façon à produire un complexe gaz-cristaux sous la forme d'une mousse de masse volumique inférieure à celle de l'huile. Ce complexe se rassemble dans la zone 6 du récipient, où il est éliminé par raclage selon la flèche C.At the outlet of the
La production des fines bulles de gaz neutre est obtenue en prélevant une fraction E d'huile clarifiée qui est amenée dans un saturateur 8, où elle est soumise à l'action d'un gaz neutre tel que l'air ou l'azote arrivant selon la flèche F sous une pression comprise entre 4 et 10 bars, avant d'être détendue à la pression atmosphérique, la durée du contactage gaz-huile dans le saturateur 8 étant approximativement égale à 30 mn. Ainsi, il se produit dans la fraction E', au sortir du saturateur 8, une formation de fines bulles d'air ou d'azote qui se dégagent dans le récipient 5 et viennent se fixer aux particules de solides en suspension dans l'huile. Selon une variante du procédé, on peut pressuriser la totalité de l'huile sortant du maturateur 3 en la faisant passer par le saturateur 8 avant de l'introduire dans la partie inférieure du récipient 5.The production of fine bubbles of neutral gas is obtained by taking a fraction E of clarified oil which is brought into a
Ainsi, on récupère, à la partie inférieure 7 du récipient 5, une huile clarifiée G dont une fraction E est recyclée vers le saturateur 8. Comme indiqué ci-dessus, le débit de cette fraction peut aller jusqu'à 300 % du débit de l'huile à traiter sortant du maturateur 3.Thus, at the
Par ailleurs, après destruction des mousses par chauffage, par exemple, on récupère environ 1,5 à 5 % d'huile contenant 1 % de cires.Furthermore, after destruction of the foams by heating, for example, about 1.5 to 5% of oil containing 1% of waxes is recovered.
Cette huile enrichie en cires peut être traitée par le procédé selon l'invention ou par des procédés habituels (décantation, centrifugation, filtration).This oil enriched in waxes can be treated by the method according to the invention or by usual methods (decantation, centrifugation, filtration).
La matière première de départ est une huile de tournesol contenant 800 ppm de cires. On prend 3 kg de cette huile qui a été soumise préalablement à une neutralisation et contient 0,4 % d'eau et 1 080-ppm de savon de soude, on l'introduit dans un bécher de 5 litres, équipé d'un agitateur, le tout placé dans une enceinte réfrigérée à 5°C pendant une durée d'environ 10 heures sous agitation continue. On transfère cette huile dans un saturateur de 4 litres équipé d'un agitateur. On soumet le saturateur à une pression de 10 bars.The starting raw material is a sunflower oil containing 800 ppm of waxes. We take 3 kg of this oil which has been subjected beforehand to neutralization and contains 0.4% of water and 1080-ppm of sodium hydroxide soap, it is introduced into a 5-liter beaker, equipped with an agitator. , all placed in a refrigerated enclosure at 5 ° C for a period of approximately 10 hours with continuous stirring. This oil is transferred to a saturator of 4 liters equipped with an agitator. The saturator is subjected to a pressure of 10 bars.
La durée de contactage est de 30 mn sous agitation permanente, la température de l'huile étant maintenue à 5°C par un serpentin se trouvant à l'intérieur du réacteur. A l'issue de cette opération, l'huile est détendue à la pression atmosphérique par transfert direct dans un bécher de 4 litres. Après une heure de décantation à + 5°C, on obtient une séparation de deux phases. A la partie inférieure du récipient, on récupère environ 2 850 g de l'huile décirée qui ne contient plus que 20 ppm de cires et O,1 % d'eau. A la partie supérieure du récipient, on récupère environ 150 g d'une mousse constituée par un complexe cires-fines bulles de gaz.The contacting time is 30 min with permanent stirring, the oil temperature being maintained at 5 ° C. by a coil located inside the reactor. At the end of this operation, the oil is expanded to atmospheric pressure by direct transfer to a 4-liter beaker. After one hour of decantation at + 5 ° C, a separation of two phases is obtained. At the bottom of the container, approximately 2,850 g of the dewaxed oil are recovered, which now contains only 20 ppm of waxes and 0.1% of water. At the top of the container, about 150 g of foam is recovered, consisting of a wax-fine gas bubble complex.
L'huile décirée peut être soit soumise aux stades suivants de raffinage, soit soumise à un nouveau cycle de traitement afin de parfaire le processus de décirage.The dewaxed oil can either be subjected to the following stages of refining, or subjected to a new treatment cycle in order to perfect the dewaxing process.
2 kg d'huile décirée obtenue selon l'exemple 1 sont traités de la même façon que pour l'exemple 1. L'huile entrant dans le cycle contenait 29 ppm de cires, 0,1 % d'eau et environ 50 ppm de savon. Après décantation, on obtient une huile dont la teneur en cires a été abaissée à 9 ppm. Cette huile est soumise aux stades suivants de raffinage (lavage, séchage).2 kg of dewaxed oil obtained according to example 1 are treated in the same way as for example 1. The oil entering the cycle contained 29 ppm of waxes, 0.1% of water and approximately 50 ppm of soap. After decantation, an oil is obtained, the wax content of which has been reduced to 9 ppm. This oil is subjected to the following stages of refining (washing, drying).
La matière première de départ est une huile de tournesol contenant 85 ppm de cires. On prend 3 kg de cette huile préalablement neutralisée et contenant 0,3 % d'eau et 1 400 ppm de savon de sodium. En appliquant le procédé de l'exemple 1, on obtient une huile décirée contenant 7 ppm de cires, 0,05 % d'eau et 52 ppm de savon. Le rendement en huile décirée est de 98,4 %.The starting raw material is a sunflower oil containing 85 ppm of waxes. We take 3 kg of this oil previously neutralized and containing 0.3% water and 1400 ppm of sodium soap. By applying the method of Example 1, a dewaxed oil is obtained containing 7 ppm of waxes, 0.05% water and 52 ppm of soap. The yield of dewaxed oil is 98.4%.
L'huile de départ est une huile de tournesol neutralisée et décolorée, contenant 700 ppm de cires, moins de 0,05 % d'eau et moins de 2 ppm de sodium. On procède de la même manière que dans l'exemple 1. On obtient une huile décirée contenant environ 60 ppm de cires résiduelles avec un rendement supérieur à 93 % d'huile décirée.The starting oil is a new sunflower oil marked and discolored, containing 700 ppm of waxes, less than 0.05% water and less than 2 ppm of sodium. The procedure is the same as in Example 1. A dewaxed oil is obtained containing about 60 ppm of residual waxes with a yield greater than 93% of dewaxed oil.
L'huile de départ est une huile brute de maïs contenant 150 ppm de cires. On procède comme indiqué dans l'exemple 1. On obtient une huile décirée contenant 50 ppm de cires résiduelles et dont les matières en suspension telles que mucilages, particules solides, etc.. sont en même temps partiellement éliminées.The starting oil is a crude corn oil containing 150 ppm of waxes. The procedure is as indicated in Example 1. A dewaxed oil is obtained containing 50 ppm of residual waxes and from which the suspended matters such as mucilages, solid particles, etc. are at the same time partially removed.
Il va de soi que ces exemples n'ont pas un caractère limitatif. Ce procédé pouvant s'appliquer à d'autres types d'huiles et à tous les stades de raffinage.It goes without saying that these examples are not limiting. This process can be applied to other types of oils and at all stages of refining.
Le rendement en huile décirée après clarification est donc de 95 % et peut aller jusqu'à environ 98,5 %.The yield of dewaxed oil after clarification is therefore 95% and can range up to approximately 98.5%.
Les huiles obtenues aux exemples 1 à 5 sont soumises aux opérations classiques de raffinage selon le cas, jusqu'au stade avant désodorisation.The oils obtained in Examples 1 to 5 are subjected to conventional refining operations as the case may be, up to the stage before deodorization.
Les échantillons ainsi obtenus sont entreposés à + 5°C pendant 24 heures ou plus.The samples thus obtained are stored at + 5 ° C for 24 hours or more.
Les résultats sont exposés dans le tableau ci-dessous :
Une huile contenant 1 % de cires provenant des mousses de décirage obtenues par le procédé selon l'invention est refroidie à 25-30°C pendant une nuit puis centrifugée. La phase lourde contenant les cires représente 12 % de l'huile ainsi traitée. La fraction légère représente environ 88 % d'huile partiellement décirée à 400 ppm de cires,pouvant être recyclée en mélange avec l'huile à traiter.An oil containing 1% of waxes from dewaxing foams obtained by the process according to the invention is cooled to 25-30 ° C overnight and then centrifuged. The heavy phase containing the waxes represents 12% of the oil thus treated. The light fraction represents approximately 88% partially dewaxed oil at 400 ppm of waxes, which can be recycled as a mixture with the oil to be treated.
On voit donc que par un traitement complémentaire des huiles provenant des mousses, on peut améliorer le rendement au décirage.It can therefore be seen that by additional treatment of the oils originating from the foams, it is possible to improve the dewaxing yield.
Claims (8)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AT81400750T ATE7306T1 (en) | 1980-05-22 | 1981-05-12 | METHODS OF TREATMENT OF VEGETABLE OILS TO IMPROVE THEIR STABILITY IN COLD. |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR8011450 | 1980-05-22 | ||
FR8011450A FR2482976A1 (en) | 1980-05-22 | 1980-05-22 | PROCESS FOR TREATING VEGETABLE OILS TO ENHANCE THEIR COLD STABILITY |
Publications (3)
Publication Number | Publication Date |
---|---|
EP0041002A2 true EP0041002A2 (en) | 1981-12-02 |
EP0041002A3 EP0041002A3 (en) | 1981-12-09 |
EP0041002B1 EP0041002B1 (en) | 1984-05-02 |
Family
ID=9242239
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP81400750A Expired EP0041002B1 (en) | 1980-05-22 | 1981-05-12 | Process for treating vegetable oils to improve their stability in the cold state |
Country Status (7)
Country | Link |
---|---|
EP (1) | EP0041002B1 (en) |
AR (1) | AR223283A1 (en) |
AT (1) | ATE7306T1 (en) |
CA (1) | CA1160643A (en) |
DE (1) | DE3163364D1 (en) |
ES (1) | ES8206617A1 (en) |
FR (1) | FR2482976A1 (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2683225A1 (en) * | 1991-10-31 | 1993-05-07 | Gattefosse Ets Sa | PROCESS FOR IMPROVING A GLYCEROLYZED OIL. |
US10349941B2 (en) | 2015-05-27 | 2019-07-16 | Covidien Lp | Multi-fire lead screw stapling device |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB962814A (en) * | 1959-10-12 | 1964-07-01 | Procter & Gamble Ltd | Winterizing hardened soyabean oils |
GB1120456A (en) * | 1964-12-14 | 1968-07-17 | Ranchers Cotton Oil | Method of separating components of oleaginous mixtures by fractional crystallization |
-
1980
- 1980-05-22 FR FR8011450A patent/FR2482976A1/en active Granted
-
1981
- 1981-05-12 EP EP81400750A patent/EP0041002B1/en not_active Expired
- 1981-05-12 DE DE8181400750T patent/DE3163364D1/en not_active Expired
- 1981-05-12 AT AT81400750T patent/ATE7306T1/en not_active IP Right Cessation
- 1981-05-19 ES ES502324A patent/ES8206617A1/en not_active Expired
- 1981-05-21 AR AR285407A patent/AR223283A1/en active
- 1981-05-21 CA CA000377981A patent/CA1160643A/en not_active Expired
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB962814A (en) * | 1959-10-12 | 1964-07-01 | Procter & Gamble Ltd | Winterizing hardened soyabean oils |
GB1120456A (en) * | 1964-12-14 | 1968-07-17 | Ranchers Cotton Oil | Method of separating components of oleaginous mixtures by fractional crystallization |
Non-Patent Citations (1)
Title |
---|
Guide de la séparation liquide-solide (P.Rivet), pub. 1981 ed. IDEXPO, Cachan, France Perry's Chemical Engineers' Handbook, 5e ed., McGraw-Hill Book Co. 1973 * |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2683225A1 (en) * | 1991-10-31 | 1993-05-07 | Gattefosse Ets Sa | PROCESS FOR IMPROVING A GLYCEROLYZED OIL. |
WO1993009211A1 (en) * | 1991-10-31 | 1993-05-13 | Gattefosse S.A. | Method for improving a glycerolyzed oil |
US5441738A (en) * | 1991-10-31 | 1995-08-15 | Gattefosse Sa | Process for improving a glycerolysed oil |
US10349941B2 (en) | 2015-05-27 | 2019-07-16 | Covidien Lp | Multi-fire lead screw stapling device |
US11510674B2 (en) | 2015-05-27 | 2022-11-29 | Covidien Lp | Multi-fire lead screw stapling device |
Also Published As
Publication number | Publication date |
---|---|
ES502324A0 (en) | 1982-08-16 |
EP0041002A3 (en) | 1981-12-09 |
AR223283A1 (en) | 1981-07-31 |
DE3163364D1 (en) | 1984-06-07 |
ES8206617A1 (en) | 1982-08-16 |
ATE7306T1 (en) | 1984-05-15 |
EP0041002B1 (en) | 1984-05-02 |
CA1160643A (en) | 1984-01-17 |
FR2482976A1 (en) | 1981-11-27 |
FR2482976B1 (en) | 1985-03-22 |
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